scholarly journals A Headspace Gas Chromatographic Method for Determination of Formic Acid Content in Isosulfan Blue and Various Drug Substances

2021 ◽  
Vol 37 (02) ◽  
pp. 321-329
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Rajarajan Govindasamy
Keyword(s):  
Sulfuric Acid ◽  
Formic Acid ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Class Iii ◽  
Drug Substances ◽  
Headspace Gas ◽  
Concentrated Sulfuric Acid ◽  
Gas Chromatographic Method

The Pharmaceutical industry uses formic acid in the manufacturing of various drug substances or API. At the time of manufacturing of API formic acid is use as an oxidizing agent. Formic acid is the simplest carboxylic acid. It also called methanoic acid.Formic acid present in API at high concentrations is very hazardous but in low concentrations is very beneficial. The developed and validated method was short, precise, cost effective and reproducible with FID detector and easy to use. The method is a selective and superficial analytical method for determination of formic acid in different drug substances. We report here the development and validation study of headspace gas chromatographic method to determine formic acid in different drug substances we are reported here. As per this method, the drug sample was dissolved in 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol (IPA) in a GC headspace vial and 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol used as a diluent. A AB-Inowax capillary column (30 m x 0.32 mm I.D. and 0.5 µm film thickness) was used under gradient conditions with FID. The formic acid peak was well separated from all other solvents that are used in synthesis of particular drug substance. The LOD and LOQof the method for formic acid are 82 ppm and 249 ppm respectively. Formic acid are low toxic class-III solvent as per ICH guideline.

A Headspace Gas Chromatographic Method for Determination of Formic acid Content in Isosulfan Blue and in Various Drugs

2021 ◽  
Vol 37 (2) ◽  
pp. 321-329
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Rajarajan Govindasamy
Keyword(s):  
Sulfuric Acid ◽  
Formic Acid ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Class Iii ◽  
Drug Substances ◽  
Headspace Gas ◽  
Concentrated Sulfuric Acid ◽  
Gas Chromatographic Method

The Pharmaceutical industry uses formic acid in the manufacturing of various drug substances or API. At the time of manufacturing of API formic acid is use as an oxidizing agent. Formic acid is the simplest carboxylic acid. It also called methanoic acid.Formic acid present in API at high concentrations is very hazardous but in low concentrations is very beneficial. The developed and validated method was short, precise, cost effective and reproducible with FID detector and easy to use. The method is a selective and superficial analytical method for determination of formic acid in different drug substances. We report here the development and validation study of headspace gas chromatographic method to determine formic acid in different drug substances we are reported here. As per this method, the drug sample was dissolved in 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol (IPA) in a GC headspace vial and 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol used as a diluent. A AB-Inowax capillary column (30 m x 0.32 mm I.D. and 0.5 µm film thickness) was used under gradient conditions with FID. The formic acid peak was well separated from all other solvents that are used in synthesis of particular drug substance. The LOD and LOQof the method for formic acid are 82 ppm and 249 ppm respectively. Formic acid are low toxic class-III solvent as per ICH guideline.

scholarly journals Identification of the Organic Volatile Impurities in Ezitamibe using GC-HS Technique

2021 ◽  
Vol 33 (3) ◽  
pp. 605-610
Author(s):  
Durgababu Rapeti ◽  
Kapavarapu Maruthi Venkata Narayanarao ◽  
Pulipaka Shyamala ◽  
Rallabhandi Murali Krishna
Keyword(s):  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Organic Chemical ◽  
Dimethyl Formamide ◽  
Flame Ionization ◽  
Drug Substances ◽  
Periodic Analysis ◽  
Ionization Mode ◽  
Gas Chromatographic Method ◽  
Volatile Impurities

Ezetimibe prevents intestinal cholesterol synthesis, which in turn reduces the quantity of cholesterol and thereby helps to reduce heart problems and strokes. In the production of ezetimibe, several organic chemical solvents such as methanol, acetone, isopropyl alcohol, dichloromethane, n-hexane, ethyl acetate, tetrahydrofuran, toluene and dimethyl formamide were used. The measurement of residual solvents is necessary for release checks of all drug substances, based on sound manufacturing processes. The analysis of above mentioned nine solvents in ezetimibe drug was investigated using gas chromatographic method employing detection with flame ionization mode. All analyses were performed using ZB-624 column (30 m length × 0.53 mm identification, 3.0 μm thickness film). The column oven temperature flux was managed to maintain for 11 min at 40 ºC and then continued to upsurge to a temperature close of 240 ºC at a rate of 20 ºC/min and retained for 4 min. The flame ionization detector and injector port were managed at 260 and 200 ºC, respectively. Results after the validation of the gas chromatographic method showed the satisfactory linearity, sensitivity, robustness, accuracy, selectivity and precision for the tested organic solvents. This gas chromatographic approach can therefore be exploited in the assessment of studied nine residual chemical solvents for periodic analysis by gas chromatography for samples of ezetimibe drug.

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